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一测多评法同时测定瑶药月里瑶秘喷雾剂中7种有效成分的含量
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| 篇名： | 一测多评法同时测定瑶药月里瑶秘喷雾剂中7种有效成分的含量 |
| TITLE： | Simultaneous Determination of 7 Effective Components in Yao Medicine Yueli Yaomi Spray by QAMS |
| 摘要： | 目的：建立一测多评（QAMS）法同时测定瑶药月里瑶秘喷雾剂中α-香附酮、α-蒎烯、β-蒎烯、柠檬烯、β-榄香烯、氧化石竹烯、藁本内酯等7种有效成分的含量，为该制剂质量控制提供方法参考。方法：采用气相色谱法进行测定。色谱柱为DB-1701P毛细管柱，载气为氮气，氢火焰离子检测器的温度为240℃，程序升温，进样口温度为240℃，进样量为1μL，分流比为20∶1。以柠檬烯为内参物，计算其余6种成分的相对校正因子，再根据相对校正因子计算出6种成分的含量，并与内标法（以萘为内标物）测定结果进行比较。结果：α-香附酮、α-蒎烯、β-蒎烯、柠檬烯、β-榄香烯、氧化石竹烯、藁本内酯检测质量浓度的线性范围分别为0.0089～1.1100、0.0283～3.5400、0.0205～2.5600、0.0230～2.8800、0.0163～2.0350、0.0131～1.6400、0.0083～1.0400mg/mL（r均大于0.9990）；定量限分别为0.0056、0.0131、0.0114、0.0186、0.0108、0.0089、0.0045mg/mL；检测限分别为0.0019、0.0041、0.0037、0.0062、0.0035、0.0029、0.0015mg/mL；精密度、稳定性（24h）、重复性试验的RSD均小于2％（n＝5或n＝6）；平均回收率分别为98.48％、101.37％、97.96％、99.80％、102.79％、97.77％、102.14％，RSD均小于2％（n＝9）。α-香附酮、α-蒎烯、β-蒎烯、β-榄香烯、氧化石竹烯、藁本内酯的平均相对校正因子分别为1.0458、0.6210、0.4885、0.3829、0.7089、0.9569，RSD均小于2％（n＝6）。QA-MS法和内标法测得的7种成分的含量差异均无统计学意义（P＞0.05）。结论：建立的QAMS法简便、准确、稳定且重现性良好，可用于月里瑶秘喷雾剂中7种成分的同时测定。 |
| ABSTRACT： | OBJECTIVE：To establish QAMS method for simultaneou s determination of 7 effective components in Yao medicine Yueli yaomi spray ，such as α-cyperone，α-pinene，β-pinene，limonene，β-elemene，caryophyllene oxide and ligustilide ， so as to provide method reference for the quality control of the preparation. METHODS ：GC method was adopted. The determination was performed on DB- 1701P capillary column ，using nitrogen as carrier gas. The temperature of the hydrogen flame ion detector was 240 ℃. The temperature was programmed ，the inlet temperature was 240 ℃，the injection volume was 1 μL and the split ratio was 20 ∶ 1. Using limonene as internal reference ，the relative correction factors of other 6 components were calculated，the contents of them were calculated with relative correction factors ，and then compared with the results of internal standard method （using naphthalene as internal standard ）. RESULTS ：The mass concentration linear range of α-cyperone， α-pinene，β-pinene，limonene，β-elemene，caryophyllene oxide and ligustilide were 0.008 9-1.110 0，0.028 3-3.540 0，0.020 5- 2.560 0，0.023 0-2.880 0，0.016 3-2.035 0，0.013 1-1.640 0，0.008 3-1.040 0 mg/mL（all r＞0.999 0）；the limits of quantification were 0.005 6，0.013 1，0.011 4，0.018 6，0.010 8，0.008 9，0.004 5 mg/mL；the detection limits were 0.001 9，0.004 1，0.003 7， 0.006 2，0.003 5，0.002 9，0.001 5 mg/mL；RSDs for precision ，stability（24 h），and repeatability tests were all less than 2％ （n＝5 or n＝6）； the average recoveries were 98.48％ ， 014） 101.37％，97.96％，99.80％，102.79％，97.77％，102.14％， and RSDs were all lower than 2％（n＝9），respectively. The average relative correction factors of α-cyperone，α-pinene， β-pinene，β-elemene，caryophyllene oxide and ligustilide were 1.045 8，0.621 0，0.488 5，0.382 9，0.708 9，0.956 9 respectively，and the RSDs were all lower than 2％（n＝6）. There wa s no statistical significance in contents of 7 components between QAMS method and internal standard method （P＞0.05）. CONCLUSIONS ：The established QAMS method is simple ， accurate，stable and reproducible ，and can be used for simultaneous determination for 7 components in Yueli yaomi spray. |
| 期刊： | 2020年第31卷第09期 |
| 作者： | 张競之，赵丹青，王正蓉，贾金艳，杨林，张升盛，刘歆蕾，伍庆，潘卫 |
| AUTHORS： | ZHANG Jingzhi，ZHAO Danqing，WANG Zhengrong，JIA Jinyan，YANG Lin，ZHANG Shengsheng，LIU Xinlei，WU Qing，PAN Wei |
| 关键字： | 一测多评法；瑶药；月里瑶秘喷雾剂；气相色谱法；质量控制 |
| KEYWORDS： | QAMS；Yao medicine ；Yueli yaomi spray ；GC；Quality control |
| 阅读数： | 351 次 |
| 本月下载数： | 5 次 |
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